CN105854809B - A kind of modified activated carbon and preparation method thereof for middle and high concentration VOCs absorption - Google Patents
A kind of modified activated carbon and preparation method thereof for middle and high concentration VOCs absorption Download PDFInfo
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- CN105854809B CN105854809B CN201610442780.4A CN201610442780A CN105854809B CN 105854809 B CN105854809 B CN 105854809B CN 201610442780 A CN201610442780 A CN 201610442780A CN 105854809 B CN105854809 B CN 105854809B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
- F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
- F23G7/00—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals
- F23G7/06—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases
- F23G7/07—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases in which combustion takes place in the presence of catalytic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/10—Inorganic adsorbents
- B01D2253/102—Carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/708—Volatile organic compounds V.O.C.'s
Abstract
The invention belongs to catalyst preparation technical field, specially a kind of modified activated carbon and preparation method thereof for middle and high concentration VOCs absorption.The present invention adds binder after crushed and mixes molding using common coconut husk as raw material, and column cocoanut active charcoal is prepared by high temperature cabonization activation, is modified by carried metal cation to it, active carbon can be improved to the adsorption capacity of VOCs.The preparation-obtained cocoanut active charcoal specific surface area of the present invention reaches 1200m2/ g, has many advantages, such as fast to organic exhaust gas adsorption desorption rate, and saturated adsorption capacity is high.The adsorbent can be widely applied for the recovery processing of organic exhaust gas, reach 90% or more to the adsorption efficiency of organic exhaust gas.
Description
Technical field
The invention belongs to catalyst preparation technical field, specially a kind of modified active for middle and high concentration VOCs absorption
Charcoal and preparation method thereof.
Background technique
Volatile organic compounds is the major pollutants of the industries such as printing, petrochemical industry, electronics, paint and pharmacy, not
Human health can also be seriously endangered by not only resulting in environmental pollution through a large amount of discharges of processing.The VOCs total amount that China is discharged every year reaches
10000000 tons or more, thus it is extremely urgent to the improvement of China VOCs.Mainly have to organic waste gas treatment method at present absorption method,
Catalysis burning winding, bioanalysis, plasma method, flame combustion method etc., but due to the VOCs content of different industries and form big phase
It is very unlike, therefore increase the difficulty of governance of VOCs.Absorption method is current China's industrial organic exhaust gas processing with most commonly used
Technology, equipment cost is low, easy to operate, adsorption efficiency is high, can be used as middle and high concentration VOCs pretreatment or subsequent place
Reason, and organic exhaust gas higher for expensive or concentration has certain economic benefit.Document is for VOCs at present
Is defined as:<200ppm is low concentration, and 200-5000ppm is intermediate concentration, and>5000ppm is high concentration.
The adsorbent of VOCs is commercially used for based on high efficiency active carbon and activated carbon fibre at present, compared with active carbon,
Activated carbon fibre has many advantages, such as large specific surface area, and adsorption desorption speed is fast, and can be easily made the form of paper, felt, the gas of generation
Resistance is smaller, but it is expensive, and technology is monopolized by overseas enterprise.Therefore durable and efficient acticarbon is prepared
Increasingly it is valued by people.Conventional cocoanut active charcoal has huge specific surface area and pore volume, to gas absorption performance
It is excellent, but its adsorptive selectivity is poor, is not able to satisfy the adsorption/desorption requirement of special VOCs.
Chinese patent CN102000548A discloses a kind of " preparation of the modified activated carbon absorbent of low-concentration organic exhaust gas
Method ", adsorbent composition are as follows: the tungsten oxide of 3-5%, perhaps iron oxide or cerium oxide and the oxidation of the cerium oxide of 0-2%
Iron, remaining ingredient are active carbon.Chinese patent CN103495386 discloses a kind of " activated carbon adsorption of low-concentration organic exhaust gas
Agent and preparation method thereof ", adsorbent weight part composition are as follows: the cerium oxide of active carbon 100-200,2-3, the ammonium persulfate of 1-2,
70-80 diatomite, the lignin of 3-4,8-10 modified attapulgite and suitable water.Although above-mentioned two invention is organic in low concentration
Certain effect is achieved on waste gas purification, but the purification and recycling for middle/high concentration organic waste gas are ineffective,
Therefore preparation is increasingly taken seriously for the adsorbent of middle/high concentration organic waste gas.
Summary of the invention
It is an object of the invention to against the above technical problems, provide a kind of modified work for middle and high concentration VOCs absorption
Property charcoal.The modified activated carbon is suitable for middle and high concentration VOCs adsorption treatment, and by itself and catalysis burning combination, improves catalysis burning
Efficiency, realize being fully cleaned up for VOCs.
Another object of the present invention is that providing the preparation method of more than one catalyst.
The object of the invention is realized by following technical proposals:
A kind of modified activated carbon for middle and high concentration VOCs absorption, first crushes coconut husk, sieves, then in mass ratio
For 1:(0.1-3) ratio and binder mix form, then be carbonized, activate prepare it is columned with certain mechanical strength
Active carbon, finally by the modified particle diameter of preparing of strong oxidizer for 3-5mm, particle length 6-15mm, specific surface area reaches
700-1300m2/ g, aperture focus primarily upon the acticarbon between 0.4-1.2nm
A kind of preparation method of the modified activated carbon for middle and high concentration VOCs absorption, comprising the following steps:
(1) it takes 1000g coconut husk to be added to dipping 12-24h in the NaOH solution of 5L 0.05-0.3g/ml to be pre-processed,
Impurity is removed, then filtration washing to neutrality, dries 12h in 100 DEG C of baking ovens；
(2) by pretreated cocoanut active charcoal in 500-1000 DEG C, 100-1000ml/min N2Under the conditions of be carbonized 1-
10h；
(3) cocoanut active charcoal after carbonization is packed into ball mill and crushes ball milling 5-30h, then sieved with 100 mesh sieve；
(4) taking in step (3) preparation-obtained 20-200g coconut shell flour and binder according to mass ratio is 1:(0.1-3)
It mixes, it is the column raw material that 3-5mm length is 6-15mm or so that 5-40ml distilled water extrusion forming, which is then added, and obtains diameter；
(5) the preparation-obtained column raw material of step (4) is solidified to drying 1-10h in 180 DEG C of baking ovens；
(6) raw material being prepared in step (5) is placed in tube furnace, in 700-1000 DEG C, 100-1000ml/
minCO2Under conditions of carry out activation 5-40h, column cocoanut active charcoal A is prepared；
(7) will be 1g:(5-30 by solid-to-liquid ratio) to be impregnated into concentration be 0.01-0.5g/ml Cu to ml cocoanut active charcoal A2+, or
Ni2+Or Zn2+Or Ce3+Or Zr4+It is quiet at a temperature of 60-90 DEG C in one of plasma or several nitrate solutions
Set 1-6h, take out filtering, add in 100ml distilled water and wash, wash at room temperature three times, then repeated impregnations twice, every time
It is washed three times after dipping.It takes out filtering and dries 12h in 100 DEG C of baking ovens again, then in 300-400 DEG C of N2Under the conditions of roast
4h obtains modified activated carbon.
In Φ 18mm, the tempering of long 60cm leads directly in reaction tube the performance evaluation for carrying out adsorbent, the amount of fill of adsorbent
For 15ml, air speed 20000h-1, adsorption reaction carries out at normal temperatures and pressures.Unstripped gas is the toluene mixed gas of 3500ppm,
Carrier gas and carrier gas are air, adsorption time 120min.Detachment assays are in 150 DEG C of N2Under the conditions of carry out, desorption air speed be
10000h-1, desorption time 120min.
The positive effect of the present invention is:
(1), the modified activated carbon that this method is prepared is adsorbed suitable for middle and high concentration VOCs, which can be with
Active carbon is improved to the adsorption capacity of VOCs.
(2), the specific surface area for the modified activated carbon that the application is prepared using coconut husk etc. as raw material reaches 1200m2/
G, has many advantages, such as fast to organic exhaust gas adsorption desorption rate, and saturated adsorption capacity is high.
(3), the adsorbent can be widely applied for the recovery processing of organic exhaust gas, reach to the adsorption efficiency of organic exhaust gas
90% or more.
Detailed description of the invention
Fig. 1 is the structural schematic diagram for the absorption detection device that embodiment part is used in the present invention.
Wherein, 1 --- mass flowmenter (gas and liquid), 2 --- miniature metering pump (band flow indication), 3 --- steaming
--- --- --- temperature indicator, 7 --- the condenser, 8 --- liquid storage of catalyst reactor, 6 of heating furnace, 5 of clouding clutch, 4
Tank.
Fig. 2 is that sample A1, A2 and B change over time curve synoptic diagram to the purifying rate of toluene in embodiment.
Specific embodiment
Foregoing invention content of the invention is described in further detail With reference to embodiment, but should not be incited somebody to action
This range for being interpreted as the above-mentioned theme of the present invention is only limitted to following embodiments.The above-mentioned technical idea situation of the present invention is not being departed from
Under, according to ordinary skill knowledge and customary means, various replacements and change are made, the scope of the present invention should all be included in
It is interior.
Embodiment 1:
1000g coconut husk is added in 5L 0.1g/ml NaOH solution and impregnates 12h, removes impurity, then filtration washing is extremely
Neutrality dries 12h in 100 DEG C of baking ovens, and the coconut husk after drying is put into 800 DEG C of 200ml/min N in tube furnace2Under the conditions of carbon
Change 3h, then the coconut husk raw material after carbonization is put into ball mill and crushes milling 12h, sieves with 100 mesh sieve son；Weigh 100g coconut husk
Powder, addition 100g soluble starch mix, and add the mixing of 30ml distilled water, and being then placed in extruder and being shaped to diameter is 3-
4mm length is the regular column raw material of 6-10mm, and the column raw material of extrusion is solidified to drying 10h in 140 DEG C of baking ovens, later will
Raw material object is put into tube furnace in 900 DEG C of 300ml/min CO2Under the conditions of activate 25h, obtain cocoanut active charcoal A1, the reality of evaluation
Test that the results are shown in Table 1.
Embodiment 2:
1000g coconut husk is added in 5L 0.1g/ml NaOH solution and impregnates 12h, removes impurity, then filtration washing is extremely
Neutrality dries 12h in 100 DEG C of baking ovens, and the coconut husk after drying is put into 800 DEG C of 200ml/min N in tube furnace2Under the conditions of carbon
Change 3h, then the coconut husk raw material after carbonization is put into ball mill and crushes milling 12h, sieves with 100 mesh sieve son；Weigh 100g coconut husk
Powder, addition 100g phenolic resin mix, and add the mixing of 30ml distilled water, and being then placed in extruder and being shaped to diameter is 3-
4mm length is the regular column raw material of 6-10mm, and the column raw material of extrusion is solidified to drying 10h in 140 DEG C of baking ovens, later will
Raw material object is put into tube furnace in 900 DEG C of 300ml/min CO2Under the conditions of activate 25h, obtain cocoanut active charcoal A2, the reality of evaluation
Test that the results are shown in Table 1.
Embodiment 3:
20g cocoanut active charcoal A1 is taken to be impregnated into 200ml 0.1g/ml Cu (NO3)2In solution, stood at a temperature of 90 DEG C
1h takes out filtering, distills water washing three times with 100ml again at room temperature, then repeats dipping twice, same after dipping every time
Three times, taking-up dries 12h in 100 DEG C of baking ovens, then in 350 DEG C of N for washing2Under the conditions of roast 4h, obtain modified activated carbon B,
The experimental result of evaluation is as shown in table 1.
Embodiment 4:
20g cocoanut active charcoal A1 is taken to be impregnated into 200ml 0.1g/ml Ni (NO3)2In solution, stood at a temperature of 90 DEG C
1h takes out filtering, distills water washing three times with 100ml again at room temperature, then repeats dipping twice, same after dipping every time
Three times, taking-up dries 12h in 100 DEG C of baking ovens, then in 350 DEG C of N for washing2Under the conditions of roast 4h, obtain modified activated carbon C,
The experimental result of evaluation is as shown in table 1.
Embodiment 5:
20g cocoanut active charcoal A1 is taken to be impregnated into 200ml 0.1g/ml Zn (NO3)2In solution, stood at a temperature of 90 DEG C
1h takes out filtering, distills water washing three times with 100ml again at room temperature, then repeats dipping twice, same after dipping every time
Three times, taking-up dries 12h in 100 DEG C of baking ovens, then in 350 DEG C of N for washing2Under the conditions of roast 4h, obtain modified activated carbon D,
The experimental result of evaluation is as shown in table 1.
Embodiment 6:
20g cocoanut active charcoal A1 is taken to be impregnated into 200ml 0.1g/ml Ce (NO3)3In solution, stood at a temperature of 90 DEG C
1h takes out filtering, distills water washing three times with 100ml again at room temperature, then repeats dipping twice, same after dipping every time
Three times, taking-up dries 12h in 100 DEG C of baking ovens, then in 350 DEG C of N for washing2Under the conditions of roast 4h, obtain modified activated carbon E,
The experimental result of evaluation is as shown in table 1.
Embodiment 7:
20g cocoanut active charcoal A1 is taken to be impregnated into 200ml 0.1g/ml Zr (NO3)4In solution, stood at a temperature of 90 DEG C
1h takes out filtering, distills water washing three times with 100ml again at room temperature, then repeats dipping twice, same after dipping every time
Three times, taking-up dries 12h in 100 DEG C of baking ovens, then in 350 DEG C of N for washing2Under the conditions of roast 4h, obtain modified activated carbon F,
The experimental result of evaluation is as shown in table 1.
Embodiment 8:
20g cocoanut active charcoal A2 is taken to be impregnated into 200ml 0.1g/ml Cu (NO3)2In solution, stood at a temperature of 90 DEG C
1h takes out filtering, distills water washing three times with 100ml again at room temperature, then repeats dipping twice, same after dipping every time
Three times, taking-up dries 12h in 100 DEG C of baking ovens, then in 350 DEG C of N for washing2Under the conditions of roast 4h, obtain modified activated carbon G,
The experimental result of evaluation is as shown in table 1.
The above sample is subjected to adsorption assessment, detection method can be detected using the prior art, can also be used
Its detection device as shown in Figure 1 is detected, concrete operation method are as follows:
1) 15ml active carbon, is measured with graduated cylinder, then it is weighed on balance again, recording its initial mass is m1,
Load weighted acticarbon is enclosed in Φ 18mm, the tempering of long 60cm leads directly in reaction tube, is then placed in reaction tube
Tube furnace connects gas circuit, is passed through the air-tightness that nitrogen checks system；
2) nitrogen flow, is adjusted to 100ml/min, and tube furnace is warming up to 350 DEG C with the rate of 5 DEG C/min, is protected
Hold 2h, in order to the water and gaseous impurity in acticarbon are removed, is down to 100 DEG C to temperature, takes out active carbon, it is right
It is sealed weighing, records its quality m2；
3), keeping tubular type furnace temperature is 30 DEG C, and load weighted active carbon is reloaded tempering and is led directly in reactor, is passed through
Nitrogen check device air-tightness, is then switched to bypass for gas circuit, and gas is made no longer to pass through reactor, opens gas-chromatography, closes
Close N2Air is opened, is 5L/min by both air flow modulation, opens miniature metering and toluene is passed into evaporation mixer, toluene
Flow velocity be 0.02ml/min, after gas flow stablize after measure toluene initial concentration, repeatedly measurement to toluene concentration stablize；
4) mixed gas, is switched into reactor, by activity, at interval of the primary outlet toluene concentration of measurement in 5 minutes, directly
Until exit concentration is close to initial concentration, micro pump is closed；
5) active carbon after absorption, is taken out, is weighed, records quality m3；
6), active carbon is reinstalled herein to stainless steel lead directly to reactor, is passed through N2Flow remains 2.5L/min, check device
Air-tightness will heat up with 5 DEG C/min to 150 DEG C, start to measure armatine benzene concentration, primary every measurement in 10 minutes, until going out
Armatine benzene concentration is zero, stops experiment, takes out active carbon and weighs, records quality m4。
Calculation formula:
The calculating of adsorption rate=(m3-m2)/m2
The calculating of desorption rate=(m3-m4)/(m3-m2)
The experimental result of adsorption assessment is as shown in table 1
The adsorpting data of 1 active carbon of table
As seen from the above table: the active carbon adsorption desorption better performances being prepared using starch as binder use metal ion
It is modified its its improve to the adsorption desorption performance of toluene, use Cu2+Saturation of the modified obtained adsorbent to toluene
Adsorption capacity and desorption rate performance are best.
Claims (2)
1. a kind of preparation method of the modified activated carbon for middle and high concentration VOCs absorption, it is characterised in that the following steps are included:
(1) it takes 1000g coconut husk to be added to dipping 6-24h in the NaOH solution of 5L 0.05-0.3g/ml to be pre-processed, goes to clean
Matter, then filtration washing to neutrality, dries 12h in 100 DEG C of baking ovens；
(2) by the coconut husk after drying in 500-1000 DEG C, 100-1000ml/minN2Under the conditions of be carbonized 1-10h；
(3) the coconut husk raw material after carbonization is packed into ball mill and crushes ball milling 5-30h, then sieved with 100 mesh sieve；
(4) preparation-obtained 20-200g coconut shell flour and binder in step (3) is taken to mix according to mass ratio for 1:(0.1-3),
Then 5-40ml distilled water extrusion forming is added and obtains column raw material；Select any one in soluble starch or phenolic resin
Or it is several as binder；
(5) the preparation-obtained column raw material of step (4) is solidified to drying 1-10h in 180 DEG C of baking ovens；
(6) raw material being prepared in step (5) is placed in tube furnace in 700-1000 DEG C, 100-1000ml/minCO2Condition
Under carry out activation 5-30h, column cocoanut active charcoal A is prepared；
(7) cocoanut active charcoal A is impregnated into the nitrate solution containing metal cation for 1g:(5-30) ml by solid-to-liquid ratio,
1-6h is stood at 60-90 DEG C, three times, then repeated impregnations twice, three times, take out filtering and exist again after dipping every time by washing for washing
12h is dried in 100 DEG C of baking ovens, then in 300-400 DEG C of N2Under the conditions of roast 4h, obtain modified activated carbon；Gold for load
Belonging to cation is Cu2+、Ni2+、Zn2+、Ce3+And Zr4+Any one or a few in ion, concentration of polymer solution 0.01-
0.5g/ml；The modified activated carbon particle diameter for using this method to be prepared is 3-5mm, particle length 6-15mm, specific surface
Product reaches 700-1300m2/ g, aperture concentrate between 0.4-1.2nm.
2. a kind of preparation method of the modified activated carbon for middle and high concentration VOCs absorption according to claim 1, feature
Be: the nitrate of metal cation is Cu (NO3)2·3H2O、Ni(NO3)2·6H2O、Zn(NO3)2·6H2O、Ce(NO3)3·
6H2O and Zr (NO3)4·5H2In O any one or it is several.
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| CN108283920B (en) * | 2017-01-09 | 2021-07-27 | 青州日新特种材料有限公司 | NOx removal catalyst and preparation method thereof |
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| CN111804272A (en) * | 2020-06-23 | 2020-10-23 | 生态环境部南京环境科学研究所 | Preparation and activation integrated device of charcoal adsorbent for organic sewage treatment |
| CN112169762B (en) * | 2020-10-27 | 2021-05-04 | 山东津挚环保科技有限公司 | Pressure swing adsorption hydrogen extraction adsorbent, preparation method and application |
| CN112354093A (en) * | 2020-11-02 | 2021-02-12 | 中国人民解放军陆军防化学院 | Multifunctional filtering tank for gas mask |
| CN113019317A (en) * | 2021-01-20 | 2021-06-25 | 桂林理工大学 | Bimetal-loaded activated carbon high-performance adsorbent and preparation method and application thereof |
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| CN102000548A (en) * | 2010-12-02 | 2011-04-06 | 上海纳米技术及应用国家工程研究中心有限公司 | Method for preparing modified active carbon adsorbent of low-concentration organic waste gas |
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|---|---|---|---|---|
| CN101780952A (en) * | 2010-03-26 | 2010-07-21 | 上海交通大学 | Method for preparing loading functional oxide porous carbon |
| CN104211043A (en) * | 2014-08-29 | 2014-12-17 | 中国人民解放军63971部队 | Preparation method of bamboo charcoal with high specific surface area |
| CN104692379A (en) * | 2014-12-24 | 2015-06-10 | 无限极（中国）有限公司 | Hemp-stem active carbon and preparation method, forming method and application thereof |
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